反应详情

温度

95 °C

1-(tert-Butoxycarbonyl)-4-(4-methylphenylsulphonyloxymethyl)piperidine (40 g, 0.11 mol), (prepared as described for the starting material in Example 1), was added to a suspension of ethyl 4-hydroxy-3-methoxybenzoate (19.6 g, 0.1 mol) and potassium carbonate (28 g, 0.2 mol) in dry DMF (200 ml). After stirring at 95° C. for 2.5 hours, the mixture was cooled to ambient temperature and partitioned between water and ethyl acetate/ether. The organic layer was washed with water, brine, dried (MgSO4) and evaporated. The resulting oil was crystallised from petroleum ether and the suspension was stored overnight at 5° C. The solid was collected by filtration, washed with petroleum ether and dried under vacuum to give ethyl 4-(1-(tert-butoxycarbonyl)piperidin-4-ylmethoxy)-3-methoxybenzoate (35 g, 89%).

1. temperaturethe mixture was cooled to ambient temperature
2. custompartitioned between water and ethyl acetate/ether
3. washThe organic layer was washed with water, brine
4. dry with materialdried (MgSO4)
5. customevaporated
6. customThe resulting oil was crystallised from petroleum ether
7. waitthe suspension was stored overnight at 5° C
8. filtrationThe solid was collected by filtration
9. washwashed with petroleum ether
10. customdried under vacuum